Aluminum dihydroxy-titanium dilactate antiperspirant



3,013,223 ALUMINUM DHYDRGXYEITANTJM DZLAC- TA'TE ANHPERSPIRANT BernardSiegal, Elizabeth, NIL, assignor to Bristol-Myers Company, New York,N.Y., a corporation of Betaware No Drawing. Filed Feb. 24, 1958, Ser.No. 716,836 7 Claims. (Cl. 167-90) This invention pertains toantiperspirant compositions and more particularly to compositions forinhibiting or retarding the flow of perspiration, comprising thereaction product of titanium lactate and an aluminum-containingmaterial.

Antiperspirants, as opposed to simple deodorants, which merely maskoffensive odors, act to eliminate or retard the flow of perspirationfrom the sweat glands. Such materials, to be useful in commercialantiperspirant formulations, must be free of any tendency to cause skinirritation or sensitization and should not stain, weaken, char orotherwise damage clothing fabric with which they come into contact inthe course of recurrent normal use.

Many prior art antiperspirants are commonly defective in one or more ofthe foregoing respects. For example, aluminum salts of strong inorganicacids, such as aluminum chloride and aluminum sulfate are effectiveantiperspirants by reason of their powerful astringent action but thesesalts, when present in effective concentrations, produce skin irritationand extensive fabric damage. Aluminum salts of some strong organic acidshave also been suggested as antiperspirants, e.g., the sulfamate,sulfonate and alkyl sulfonates. Aluminum salts of other organic acids,previously suggested as antiperspirants, include the aluminum salts ofsuch sulfonated organic acids as the phenolsulfonate (sulfocarbolate),the sulfoacetate, the methionate (methane disulfonate) or salts ofWeaker organic acids, such as the acetate, lactate, acetotartrate,formate and palmitate. Various aluminum hydroxide derivatives have alsobeen used or advanced as antiperspirants, e.g., aluminum chlorhydroxide,aluminum calcium chlorhydroxide complex, and aluminumchlorhydroxyacetate. Th aluminum salts of the weaker organic acids'havebeen found to be inferior in their antiperspirant activity as havecertain of the aluminum hydroxide derivatives. Others of the lattertype, notably aluminum chlorhydroxide, although efiicientantiperspirants, result in appreciable degrees of fabric damage andstaining. The staining produced by aluminum chlorhydroxide and similarmaterials is believed to be due to a deposition upon the clothing fabricof aluminum hydroxide. The latter material, being relatively insolublein water, is not removable by washing. This tendency to cause insolublestains, together with the corrosive nature of the aluminum salts ofstrong acids, constitutes a major disadvantage when aluminum-containingcompounds are considered for incorporation in antiperspirantcompositions.

Therefore it is an object of the present invention to provide analuminum-containing compound having a high antiperspirant activity butwhich does not possess the corrosive properties of prior art aluminumcompounds.

It is another object of the present invention to provide an effectiveantiperspirant composition which is free from any tendency to stain orotherwise damage clothing fabrics.

It is a further object of the invention to provide analuminum-containing antiperspirant composition which is free from anytendency to irriate or sensitize the skin.

It is still another object of the invention to provide an antiperspirantand deodorant compound which is watertates Patent 3,i8,223 Patented Jan.23, 1962 soluble and compatible with the usual ingredients ofantiperspirant cosmetic compositions.

Other objects and advantages of the invention will appear in thefollowing description.

It has been disclosed in co-pending patent application Serial No.691,131, of E. L. Saul and B, Siegal, filed October 21, 1957, that thetitanium salts of lactic acid, hereinafter termed titanium lactate,possess antiperspirant activity. It has now been found that titaniumlactate may be reacted with an aluminum-containing material to produce areaction product, hereinafter referred to as aluminum titanium lactate,which possesses an antiperspirant activity substantially equal to orgreater than most prior art antiperspirants with the exception of themore corrosive aluminum salts such as aluminum chloride or aluminumsulfate. However, aluminum titanium lactate exhibits few or none of thedefects commonly found in such prior art antiperspirants. Aluminumtitanium lactate is water-soluble and therefore lends itself readily toincorporation in aqueous based cosmetic compositions. Moreover,antiperspirant compositions containing aluminum titanium lactate do notirritate or sensitize the unbroken skin when repeatedly applied thereto.

It has also been found that aluminum titanium lactate may be prepared ina number of difierent ways. A preferred method of preparing aluminumtitanium lactate comprises reacting titanium lactate and aluminumhydroxide. For example, the following procedure was utilized inpreparing an aluminum titanium lactate suitable for incorporation in anantiperspirant composition.

Fourteen (14) grams of titanium lactate powder were added to water in asufiicient quantity to dissolve the titanium lactate. To the titaniumlactate solution was added 20.33 grams of commercial aluminum hydroxidegel and the mixture stirred with heating to about C. until the reactionwas substantially complete as indicated by the substantially completedisappearance of the insoluble aluminum hydroxide, A suitable titaniumlactate is that manufactured and sold by the E. I. du Pont de Nemours &Co. under the trademark Tilac. A suitable aluminum hydroxide gel ismanufactured and sold by the Reheis Co. under the designation AluminumHydroxide Wet Gel F500. The latter material contains about 9 percent byweight of aluminum oxide, A1 0 20.33 grams of the aluminum hydroxide gelthus contains about 1.83 grams of A1 0 This reaction resulted in theproduction of about 15.0 grams of aluminum titanium lactate in anaqueous solution. Such solutions may be used directly for thepreparation of antiperspirant cosmetic compositions or they may beconcentrated to any desired degree.

Suitable compositions have also been prepared in a similar manner usingother commercially available aluminum hydroxide wet gels, such as ReheisWet Gel F1000 containing from 9.5 to 10.5 percent by weight of aluminumoxide or Reheis Wet Gel F2000 containing from 12.5 to 13.5 percent byweight of aluminum oxide. Dried aluminum oxide gels may also beutilized, useful products having been obtained by reacting titaniumlactate in water solution with Reheis Dried Gel F2000, containing aminimum of 50 percent by Weight of aluminum oxide and Reheis Dried GelF1000, containing a minimum of 51.5 percent by weight of aluminum oxide.

Aluminum titanium lactate may also be prepared by the reaction, inaqueous solution between titanium lactate and an aluminum alkoxide, suchas the methoxide, ethoxide, isopropoxide or t-butoxide. Thus, aluminumtitanium lactate has been prepared by slowly adding aluminum isoproxideto an aqueous solution containing 40 percent, by weight thereof, oftitanium lactate. The

reaction proceeds at ordinary temperatures until completion as indicatedby the appearance of a precipitate of aluminum hydroxide caused byreaction of an excess of aluminum isopropoxide with water. Before theend point of the reaction is reached, the reaction mass remains cleardue to the substantially instantaneous reaction with titanium lactate ofthe aluminum hydroxide produced by the decomposition of the aluminumalkoxide when contacted with Water.

Another useful procedure for the preparation of aluminum titaniumlactate comprises reacting titanium lactate with a complex compound ofan aluminum alkoxide chelated with an alkyl ester of a betaorgamma-ketocarboxylic acid. Suitable esters include the alkyl esters ofacetoacetic acid or acetopropionic acid (levulinic acid). Both of thelatter compounds have been chelated with aluminum isopropoxide and thechelated aluminum compound reacted, in aqueous solution, with titaniumlactate to produce a water-soluble reaction product which possessesmarked antiperspirant activity.

Still other aluminum compounds have been used in the preparation ofaluminum titanium lactate. For example, an aqueous solution containing15.2 grams of titanium lactate was partially neutralized to a pH ofabout 5.5 and 6.1 grams of anhydrous aluminum sulfate were added withagitation and heating to about 50 C. with the production of about 12.2grams of aluminum titanium lactate. The latter material has beenprepared in a similar manner with other aluminum salts substituted foraluminum sulfate. Thus, aluminum chloride, aluminum nitrate, aluminumsulfamate, aluminum chlorhydroxyacetate, aluminum sulfocarbolate andaluminum thiocyanate have all been used to prepare aluminum titaniumlactate. For example, in the case of each of these aluminum salts, anaqueous solution containing 15 percent, by weight thereof, of titaniumlactate was prepared and adjusted to a pH of about 7.0 by the additionof a suitable alkaline material, such as sodium hydroxide. Approximately15 grams of sodium hydroxide were required per 100 grams of titaniumlactate. To the partially neutralized titanium lactate solutions therewas added, in the case of each of the aluminum salts, 5 percent, byweight of solution, of the aluminum salts and the solution was heated,with agitation to about 50 C. Addition of the acid salts lowered the pHvalues of the solutions to between about 2.7 and 3.2, depending upon thesalt used.

These reaction masses may be used directly in the preparation ofantiperspirant formulations. Each was found to have a high order ofantiperspirant activity and, with the exception of the compositionsprepared with aluminum chloride and with aluminum nitrate, to besubstantially free of any tendency to damage fabric. The compositionscontaining the products of the reaction between titanium lactate andaluminum chloride or aluminum nitrate were found to possess sometendency to cause a weakening of fabric tensile strength. It is believedthat this tendency is due to the presence, in the unpurified reactionmasses, of the chloride and nitrate ions. The observed fabric weakeningis not greaterthan that produced by prior art antiperspirantcompositions containing these ions.

A still further procedure for preparing aluminum titanium lactatecomprises the reaction of metallic aluminum, for example, in a powder ordust form, with titanium lactate in an aqueous solution. The titaniumlactate concentration may vary from a fraction of a percent by weight ofsolution to substantial saturation, the amount of titanium lactatepreferably being slighly in excess of the stoichiometric amount in orderthat completion of the reaction may become evident by the disappearanceof the aluminum metal. Using aluminum powder, a temperature of 100 C.and a reaction time of 24 to 36 hours has been found to result in a sub-4 stantially complete reaction of stoichiometric amounts of reactants.

It is believed that the reaction product of each of the aforementionedreactions is a compound wherein two aluminum atoms are combined withthree titanium lactate moieties according to the following structuralformula:

II o H CH3 3 This material, the aluminum salt of titanium lactate,herein termed aluminum titanium lactate, is more correctly identified asaluminum dihydroxytitanium dilactate. My belief that the foregoingformula accurately represents the chemical structure of the products ofthese reactions is substantiated by the results of quantitativeanalyses. Thus, a reaction mass was prepared by reacting, in 200milliliters Water, 0.7 gram of aluminum dust and 11.6 grams of theaforementioned DuPont Tilac material which contained, by analysis, 86.5percent by weight of titanium lactate. The reaction was continued, on asteam bath, for a period of approximately two and one-half weeks inorder to insure con-- pletion of the reaction. Assuming that thereaction product, aluminum titanium lactate has the postulated molecularstructure consisting of two aluminum atoms and three titanium lactatemoieties and having a molecular weight of 834, the theoreticalconcentration of aluminum titanium lactate was 6.50 percent by weight ofthe reaction mass, i.e., 65 mg./ml. Titanium was separated and analyzedby the standard cupferron (ammonium N-nitrosophenylhydroxylamine)method, giving, for four separate analyses, an average titanium dioxideconcentration of 1.980 percent by weight of solution. Based upon thepostulated molecular structure, this corresponds to an average aluminumtitanium lactate concentration of 6.88 percent, a deviation from thetheoretical value which is within the limits of unavoidable experimentalerror.

Since the postulated three titanium lactate moieties contain a total ofsix reactive hydroxyl hydrogen atoms, it seems certain that twotrivalent aluminum atoms are required per molecule of aluminum titaniumlactate. This assumption is further substantiated by a representativelaboratory experiment wherein a 1.0727 gram portion of the same aluminumdust-titanium lactate reaction product was titrated with 0.1 N sodiumhydroxide solution. This titration gave a generally S-shaped titrationcurve, the data for which are given in Table I.

A curve erected upon the data of Table I shows two separate inflectionpoints, at pH values of approximately 7.2 and 10.3 corresponding,respectively, to alkaline volumes of 2.50 ml. and 5.00 ml. This doubleinflection in the titration curve is believed to result from theneutralization, at each inflection point of one-half of the compoundbeing titrated. Moreover the concentration of aluminum titanium lactatecalculated from the data of Table I is 6.46 percent by weight ofsolution, which agrees, within the limits of experimental error, withthe theoretical value for a molecule of the postulated structure.Similar analyses of aluminum titanium lactate made in accordance withthe other procedures described herein also give results which indicatethat the actual structure of aluminum titanium lactate is substantiallyas postulated.

Inasmuch as aluminum titanium lactate is extremely soluble in water, itsantiperspirant properties may be utilized to advantage by dissolving thecompound in water or other suitable solvent, such as water-alcoholmixtures. Such compositions containing upwards of from about 5 percentby weight thereof of aluminum titanium lactate are especially useful andthose having an aluminum titanium lactate concentration of from about toabout 20 percent by weight are particularly desirable, an aluminumtitanium lactate concentration of about percent by weight beingpreferred. The pH of a substantially impurity-free aqueous solution ofaluminum titanium lactate varies very little with concentration. Thus,the pH of aqueous solutions containing from about 5 to about 45 percentby weight of aluminum titanium lactate has been observed to vary betweenabout 3.8 and about 4.0.

The aqueous reaction masses containing aluminum titanium lactate may beused directly in the preparation of antiperspirant compositions.Moreover, it is not necessary that the reactants be present instoichiometric amounts. Thus, highly useful compositions may be producedby using less than the stoichiometric amount of aluminum-containingmaterial, thereby resulting in mixtures of aluminum titanium lactatewith titanium lactate and/ or the neutralized salts thereof.

Fabric damage tests show that, with the aforementioned exception inrespect to compositions containing chloride or nitrate ions,compositions containing aluminum titanium lactate, as well ascompositions containing mixtures of aluminum titanium lactate withtitanium lactate and/or a neutralized salt thereof, such as sodiumtitanium lactate, exhibit very little fabric damage, and, in thisrespect, represent a marked advance over a great many prior artantiperspirant compounds. Thus, tests were performed comparing theweight load necessary to break fabrics treated, on the one hand, withthe novel compositions of this invention, and, on the other hand, withaluminum chlor'nydroxide, a common ingredient in commercialantiperspirant compositions. These tests, given in Table H below, wereperformed with an Amthor Tensile Strength Tester, Type 254, sold byAmthor Testing Instrument Co., Inc. of Brooklyn, New York. The testingmachine was set for a capacity of O to 100 lbs. Ten (10) strips ofcotton fabric measuring inches x 4 inches, were used for each testsolution and the average loss of tensile strength determined. In TableII the breaking load is given in arbitrary scale units and theconcentrations of the test compositions, which are simple aqueoussolutions, are expressed in percent by weight.

It will be noted that the reduction of the average percent loss ofstrength of the fabrics treated with the novel compositions of theinvention, as compared to the fabrics treated with aluminumchlorhydroxide, varies from over eight-fold for a composition comprisinga 5050 mixture of titanium lactate and aluminum titanium lactate tosixty-fold for a composition comprising aluminum titanium lactate. ThepH of the aluminum chlorhydroxide solution used for the tests reportedin Table II was about 3.9. The pH of the aluminum titanium lactatesolutions was about 4.0 and that of the mixtures of aluminum titaniumlactate and titanium lactate was about 3.2.

The aluminum titanium lactate used in the test compositions of Table IIwas prepared by reacting with titanium lactate Reheis Aluminum HydroxideWet Gel F500. The aluminum titanium lactate compositions of Table IIcontain antiperspirant compounds in the amount of only 15 percent, ascompared to the aluminum chlorhydroxide composition which contained 20percent of the antiperspirant compound. However, it has been found that,in the case of compositions containing aluminum titanium lactate aloneor in admixture with titanium lactate or mixtures of titanium lactateand the sodium salt thereof, where the aluminum titanium lactateconstitutes at least about 50 percent by weight of the totalantiperspirant ingredients, an increase of total antiperspirant contentabove about 15 percent does not increase antiperspirant activity to adegree sufiicient to economically warrant the use of substantiallyhigher concentrations. On the other hand, current commercial aluminumchlorhydroxide-contain'mg antiperspirant compositions commonly utilizeabout 20 percent by weight of the active ingredient. Hence, the datagiven in Table II represent realistic comparisons of practical value. Anaverage loss of 20 percent, as determined by this particular test, isconsidered acceptable by nationally recognized standards.

In determining the relative freedom from damage of clothing fabricstreated with compositions of the invention as compared to the damagecaused by several prior art compositions, such as aluminum chloride,aluminum sulfate and aluminum chlorhydroxide, further tests wereemployed to duplicate actual use conditions. Thus, samples of cottonfabric were washed, rinsed, dried, ironed, and then treated withpredetermined amounts of test compositions. The treated cloth was thendried under controlled conditions and inspected for damage after whichit was again rinsed with water, dried, ironed and again inspected fordamage. Using such a test procedure, it was shown that theantiperspirant compositions containing aluminum titanium lactate weresubstantially free from any tendency to damage fabric incontradistinction to the prior art antiperspirants tested which resultedin various degrees of severe fabric damage.

A similar use test procedure was established to determine the fabricstaining propensities of the compositions of the invention and thesetests showed that the compositions are essentially free of any tendencyto stain fabrics to which they are applied. Whatever slight staining iscaused by the novel compositions of the invention is easily removable bywashing the fabric with water due to the high degree of water-solubiL tyof these compositions.

Other fabrics may be substituted for the cotton fabric in the abovetests with similar results.

The *antiperspirant activity of aluminum titanium lactate has beenestablished by a great number of human in vivo tests. For example, theresults of the topical application to the skin of aluminum titaniumlactate, in a simple water solution containing 15 percent by weight ofthe antiperspirant compound, are given in Table III wherein theantiperspirant activity of aluminum titanium lactate is compared to thatof aluminum chlorhydroxide, an effective antiperspirant in common use,and also to that of a partially neutralized aqueous solution of titaniumlactate. The compositions containing the latter two compounds were alsoin the form of aqueous solutions containing 15 percent by weight of theactive ingredient.

TABLE III TABLE V Composition Titanium LactnterAlurninum TitaniumLactate Ratio Subject No. Subject No. Aluminum Aluminum Partially Chlor-Titanium N eutrali zed 1:1 1/3:'1 0:1 hydroxide Lactate Titanium LactateThe antiperspirant activities of the test solutions were established bymeans of a standardized test procedure wherein an area of the forearm ofa test subject was exposed for 1 hour to the test solution contained inan inverted cup which was held against the arm. The forearm was thenwashed and an anhydrous mixture containing castor oil, iodine and starchwas applied whereupon a dark blue spot appeared at the site of eachactive sweat gland.

The measurement of antiperspirant activity depends on many variables, anumber of which depend on the individual test subject and are thereforenot susceptible to easy reproduction in a large test population. Inorder to minimize this dilficulty, the activity values given in TableIII are based upon the measured activity, for each individual testsubject, of aluminum chlorhydroxide. The activity of the latter compoundwas arbitrarily assigned a value of 100, hence the antiperspirantactivity values of a test composition may be determined by use ofEquation I:

a=100x/N (I) where a is the activity value of the composition undertest, x is the number of dark spots observed in ,an area of a certainsize treated with the test composition and N is the number of dark spotsproduced in an area of an equal size treated with aluminumchlorhydroxide.

The partially neutralized titanium lactate composition of Table III hada pH of 3.2 and consisted of a mixture of titanium lactate and itssodium salt in a ratio of about 66 parts of titanium lactate to about 34parts of the sodium salt.

Table IV shows that aluminum titanium lactate in a concentration ofabout percent by weight is comparable in antiperspirant activity tohigher concentrations of the other antiperspirant compounds of TableIII. Thus, in the compositions of Table IV, the aluminum titaniumlactate compositions had an active ingredient concentration of 15percent whereas the compositions containing aluminum chlorhydroxide andtitanium lactate-sodium titanium lactate mixtures had active ingredientconcentrations of percent.

The antiperspirant effectiveness of compositions containing bothaluminum titanium lactate and titanium lactate is illustrated in Table Vwherein the activities are given for aqueous compositions containing 15percent by weight of total antiperspirant, and having titanium lactate:aluminum titanium lactate ratios of 1:1, 1/3:1 and 0.1 respectively. Ineach instance, the reported activity is in reference to a standardaluminum chlorhydroxide activity value of 100.

TABLE VI Test No Composition I Activity 1 {12% Aluminum titanium lactate1 100 3% Partially neutralized titanium lactate-..

(a) 12% Aluminum titanium lactate 1 89 2 3% Partially neutralizedtitamum lactate- (b) 12% Aluminum titanium lactate 100 3% Titaniumlactate 3 {12% Aluminum titanium lactate Z 3% Titanium lactate (a) 12%Aluminum titanluml tate 3 %Titanium lactate 4 (b) 7.5% Aluminum titaniumlactate 95 7.5% Titanium lactate (c) 15% Aluminum titanium lactate LReaction product of titanium lactate and aluminum sult 2 Reactionproduct of titanium lactate and alummum oxide.

The material designated in Table VI as Partially neutralized titaniumlactate was actually present as a mix ture of titanium lactate and themono-sodium salt thereof clue to the equilibrium between these speciesat the pH of the solution. The relative amounts of titanium lactate andthe sodium salt at the specified pH are determinable by the proceduredisclosed in the aforementioned copending patent application Serial No.691,131. Thus, the specific Partially neutralized titanium lactatecomposition given in Table VI, consisted of a mixture of about 66 partsby Weight of titanium lactate to about 34 parts of mono-sodium titaniumlactate.

Although the observed test results reported in Tables III-VI show, insome instances, antiperspirant activities for the novel compositionsless than that of the reference material, aluminum chlorhydroxide, itshould be recognized that in tests of this nature the measurableantiperspirant activities are subject to wide limits of experimentalerror. Moreover, even if the observed values accurately represent theactual activity values of the novel compositions, these values aresubstantial and are soiliciently great to make the use of thesematerials desirable in antiperspirant formulations. Moreover theextremely small extent of any deleterious eifects upon clot-hing fabricto which the novel compositions are applied renders these compositionshighly superior to many prior art compositions which result in varyingdegrees of severe fabric damage or staining.

Furthermore, although many prior art antiperspirants are highlyirritating to the skin, the novel compositions of the invention havebeen found to be free of such defects. Thus, Draize repeat insult patchtest studies were performed wherein a cosmetic formulation, having anantiperspirant content in accordance with compositions 1 and 2(a)of'Table VI, was successively applied to the intact skin of 25 humansubjects on alternate days for a total of 15 applications, eachapplication being of 48 hours duration. The cosmetic vehicle was thatgiven in Example IV hereinbelow. No irritation or sensitization wasobserved.

Various forms of antiperspirant formulations, other than simple watersolutions may be prepared by utilizing, as the active antiperspirantingredient, the novel compositions of the invention. For example,cosmetic formulations in the form of creams, alcohol sprays, clear oremulsified lotions and semi-solid sticks may be made. The cream andlotion formulations may be in the form of thickened aqueous compositionsor, if desired, they may be in the form of emulsions of either thewater-in-oil or oil-in-water type, wherein the antiperspirant componentis dissolved in the aqueous phase. The oil phase of such emulsions maycomprise materials commonly used in the cosmetic arts, such as naturalsynthetic oil, fats or waxes, such as mineral oil, various vegetableoils, polyglycols, silicon es, stearic acid, cocoa butter, lanolin,paraffin, ceresin wax, spermaceti, beeswax,.a higher fatty alcohol, suchas cetyl alcohol, glycostearin, certain polyethylene glycols or varioussynthetic hydrocarbon waxes. Any compatible emulsifying agent may beutilized to stabilize such emulsions and may be, for example, of thenon-ionic type such as partial esters of fatty acids with glycerol,glycols or other polyhydric alcohols, the polyoxyethylene ethers,polyoxyethylene glycol fatty acid esters, sorbitan esters of fatty acidsand polyethylene propylene oxides. Anionic emulsifiers are also useful,for example, alkali metal, alkaline earth metal or amine salts of alkylsulfuric acid, such as sodium laurylsulfate, magnesium laurylsnlfate ortriethanolamine laurylsulfate. The emulsifiers may also be of thecationic type such as various salts of polyoxyethylene amines. Suitablehumectants, perfumes or coloring matter may be added as desired. Variousdevices of suitable nature may be utilized for the packaging anddispensing of these compositions. For example, roller type dispensersare admirably suited for the packaging and dispensing of the lotion andemulsion type formulations. The relatively fluid water and water-alcoholbased formulations may be effectively packaged in pressurized containersand dispensed therefrom in the form of aerosols, foams or liquid dropsor streams.

Useful antiperspirant formulations including aluminum titanium lactateare described in the following specific examples wherein the amounts ofthe various ingredients are given in percentage by weight.

A trademark of Atlas Powder Co., Wilmington, Delaware, for apolyoxyethylene ether.

The composition of Example I is an alcohol spray and may be prepared byforming an aqueous solution of aluminum titanium lactate by the aluminumoxide or aluminum metal method described hereinabove. Thepolyoxyethylene ether is dissolved in the remainder of the water and theglycerine, alcohol, the trichlorophenol derivative and perfume areadded, each ingredient being dissolved before the next is added. Thelatter solution is then added, with stirring, to the aluminum titaniumlactate while stirring and dissolving each ingredient before the next isadded.

Example II Component Percent Aluminum titanium lactate 12.0 Sodiumtitanium lactate 3.0 Sodium sulfate 5.0 Glyceryl monostearate 20.0 Cetylpalmitate 3.0 Petrolatum 2.0 Cetyl alcohol 1.5 Beeswax 1.0 Glycerine 4.0Perfume 0.3 Water 48.2

The formulation of Example II is a cream and may be prepared by heatingthe glyceryl monostearate, cetyl palmitate, petrolatum, cetyl alcoholand beeswax to 75 C. with stirring until melted. The glycerine isheated, to gether with a portion of water, to 75 C. and this mixture isadded to the aforementioned non-aqueous mixture with continuousstirring. To the remaining portion of the Water there is added 15 grams,per 100 grams of the final composition, of sodium titanium lactate,together with 5 grams, per 100 grams of the final composition, ofaluminum sulfate and the solution heated to 50C. The aluminum sulfatethereby reacts with a portion of the sodium titanium lactate to formabout 12 grams of aluminum titanium lactate and 5 grams of sodiumsulfate, the sodium titanium lactate remaining unreacted to the extentof about 3 grams. The solution containing aluminum titanium lactate isthen added to the emulsion and the mixture cooled with stirring to 40 C.at which point the perfume may be added.

Example III Component: Percent Aluminum titanium lactate 15.0 Glycerylmonostearate 3.5 Brij 35 3.5 Perfume 0.3 Water 77.7

The composition of Example 111 is an emulsified lotion and may beprepared by heating a portion of the Water to C. and adding thereto withstirring the glyceryl monostearate and the fatty ether derivative. Theresulting emulsion is cooled to 50 C. at which time the remainder of theWater containing the aluminum titanium lactate dissolved therein isadded with stirring. The mixture is then cooled to 40 C. and the perfumeadded.

A trademark of Atlas Powder (30., Wilmington, Delaware, forpolyoxyethylene sorbitan fatty acid ester.

The formulation given in Example IV is a clear lotion and may beprepared by dispersing the hydroxyethylcellulose in a portion of theWater with stirring. The fatty ester and perfume are dissolved in theremaining water in which the aluminum titanium lactate is alsodissolved, and this solution is then added, with stirring, to thedispersion.

1 1 Example V Components: Percent Aluminum titanium lactate 15.0 Emcol64 1 25.0 Ethanol 20.0 Propylene glycol 2.0

Polyethylene glycol (average molecular weight 350) 6.0 Perfume 0.3 Water31.7

A trademark of Emulsol Corp., Chicago, Illinois, for a fatty acid aminecondensate.

The formulation of Example V is a semi-solid cream stick and may beprepared by melting fatty acid amine condensate and adding thereto thepropylene glycol and polyethylene glycol while maintaining the mixtureat a temperature of 63 C. To this mixture is added, with stirring, asolution of the aluminum titanium lactate in the water Which has beenheated to 65 C. This solution may be prepared by adding to the Waterabout 14.0 grams of titanium lactate and about 3.7 grams of Reheisaluminum hydroxide Dried Gel No. F2000, the latter containing a minimumof 50 percent by weight of aluminum oxide. These materials react to formabout 15 grams of aluminum titanium lactate. The alcohol and perfume arethen added and the mixture stirred until homogeneous after which it maybe poured into stick molds at a temperature from about 60 to about 63 C.

It is to be understood that the foregoing examples and description aregiven merely to illustrate the novelty and utility of the invention andare not to be construed as limiting the broad principles thereof whichmay be modified by those skilled in the art without departing from thespirit and scope of the invention.

What is claimed is:

1. Aluminum dihydroxytitanium dilactate.

2. An antiperspirant composition comprising aluminum dihydroxytitaniumdilactate and a carrier therefor.

5 3. An antiperspirant composition comprising aluminum dihydroxytitaniumdilactate and an aqueous carrier therefor.

4. An antiperspirant and deodorant composition comprising a cosmeticaqueous-containing carrier having as the active ingredient anantiperspirantly effective amount of aluminum dihydroxytitaniumdilactate dissolved in the aqueous portion thereof.

5. A composition according to claim 4 wherein the aluminumdihydroxytitanium dilactate comprises at least about 5 percent by weightof the aqueous portion of the carrier.

6. The method of inhibiting perspiration which comprises applying to theskin a composition comprising aluminum dihydroxytitanium dilactate.

7. The method of inhibiting perspiration which comprises topicallyapplying to the skin an aqueous composition comprising at least about 5percent, by weight of the composition, of aluminum dihydroxytitaniumdilactate.

References Cited in the file of this patent UNITED STATES PATENTS2,236,387 Wallace Mar. 25, 1941 2,707,667 Severn May 3, 1955 OTHERREFERENCES Grote: Drug and Cos. Ind. 59:6, December 1946, pp. 776, 777,872-875. De Navarre: The Chemistry and Manuf. of Cosmetics,

D D. Van Nostrand Co., New York, 1941, page 261.

UNITED STATES PATENT OFFICE CERTIFICATION OF CORRECTION Patent No. 3 018a 223 Bernard Siegal January 23, 1962 It is hereby certified that errorappears in the above numbered patent requiring correction and that thesaid Letters Patent should read as corrected below.

Column 1 line 69, for "irriate" read irritate column 2, line 71 for"isoproxide" read isopropoxide column 3, line 70, for "slighly" readslightly column 4, lines 7 to 15, the structural formula should appearas shown below instead of as in the patent:

column 7, lin e 41, for "sodium" read mono-sodium Signed and sealed this26th da of June 1962,

(SEAL) Attest:

ERNEST W. SWIDER Attesting Officer DAVID L. LADD Commissioner of Patents

1. ALUMINUM DIHYDROXYTITANIUM DILACTATE.
 2. AN ANTIPERSPIRANT COMPOSITION COMPRISING ALUMINUM DIHYDROXYTITANIUM DILACTATE AND A CARRIER THEREFOR. 